CN111254293A - Preparation purification treatment and purification effect evaluation method of aluminum foil blank - Google Patents
Preparation purification treatment and purification effect evaluation method of aluminum foil blank Download PDFInfo
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- CN111254293A CN111254293A CN202010062144.5A CN202010062144A CN111254293A CN 111254293 A CN111254293 A CN 111254293A CN 202010062144 A CN202010062144 A CN 202010062144A CN 111254293 A CN111254293 A CN 111254293A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B21/00—Obtaining aluminium
- C22B21/06—Obtaining aluminium refining
- C22B21/066—Treatment of circulating aluminium, e.g. by filtration
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B21/06—Obtaining aluminium refining
- C22B21/062—Obtaining aluminium refining using salt or fluxing agents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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Abstract
The invention discloses a method for preparing and purifying aluminum foil blanks and evaluating the purifying effect of the aluminum foil blanks, which comprises the following steps: primary purification treatment: putting the aluminum foil blank into a smelting furnace, adding a purifying agent and a refining agent, taking the aluminum slag out of the surface of the aluminum liquid, uniformly melting, preserving heat, adding a degassing agent, standing, and slagging off for the first time; secondary purification treatment: scattering a purifying agent into the aluminum liquid subjected to primary slagging-off, stirring, standing, and performing secondary slagging-off; pouring treatment: pouring the aluminum liquid subjected to secondary purification treatment; homogenizing: carrying out homogenization annealing treatment on the cast aluminum foil blank; thermoplastic deformation treatment: the impurity content, the impurity removal rate and the average grain size are measured, the preparation and purification treatment method can effectively improve the original structure and the thermal compression deformation structure form of the aluminum foil blank, and finally improve the mechanical property of the aluminum foil blank material, so that the aluminum foil blank has high purity, less impurities, smaller grain structure size and uniform distribution.
Description
Technical Field
The invention relates to the field of forming control of non-ferrous alloys, in particular to a method for preparing and purifying aluminum foil blanks and evaluating the purifying effect of the aluminum foil blanks.
Background
The aluminum foil blank is pure aluminum alloy, represented by 1235 aluminum alloy, the purity of the aluminum foil blank is more than 99.0 percent (mass), wherein Si and Fe are main alloy elements, the aluminum foil blank is mainly used for aluminum foil products, and the aluminum and aluminum alloy plate strips with the thickness of less than 0.2mm are produced by the aluminum foil in a pressure processing mode and are widely applied to the fields of food packaging, containers, buildings and the like. This alloy has the lowest strength (of the aluminum alloys) and cannot be heat-treated for strengthening, so that cold working is used to improve its mechanical properties: high plasticity in an annealing state, good plasticity in semi-cold-work hardening, low plasticity in cold-work hardening and poor machinability.
The thickness of the aluminum foil is further reduced to obtain a high-quality aluminum foil product, and the aluminum foil blank has a reasonable organization structure through reasonable alloy design and process optimization so as to reduce the deformation resistance of the material as much as possible, reduce the work hardening rate and improve the rolling performance of the aluminum foil blank.
The gas, various inclusions and the like in the melt cause defects of pores, looseness, non-metallic inclusions, oxide films and the like of the cast ingot, and have obvious influence on the strength, the processing performance, the corrosion resistance, the anodic oxidation performance and the appearance quality of products. Therefore, the purification treatment of the aluminum melt is the key point for reducing the gas content and non-metallic inclusions of the aluminum melt and improving the quality of the processed material. The traditional aluminum liquid purification treatment process is generally operated in batches in a heat preservation furnace, and nitrogen-chlorine mixed gas and a fusing agent are generally adopted for refining. The purification treatment process is mostly operated manually, the degassing rate is low, the refining is not thorough, and the aluminum liquid is polluted again in the process of conveying the aluminum liquid from the holding furnace to the casting machine, so that the material has more defects such as impurities, air holes, microcracks and the like, the plastic deformation is influenced, and the rejection rate is increased; secondly, the material has a coarse grain structure, uneven structure during hot working, easily produces lug making during deep drawing and has poor plastic deformation performance.
Disclosure of Invention
The invention aims to overcome the defects and provides a preparation purification treatment and a purification effect evaluation method of an aluminum foil blank.
In order to achieve the purpose, the technical solution of the invention is as follows: a preparation and purification treatment method of an aluminum foil blank comprises the following steps:
primary purification treatment: putting the aluminum foil blank into a smelting furnace, adding a purifying agent and a refining agent, taking the aluminum slag out of the surface of the aluminum liquid, uniformly melting, preserving heat, adding a degassing agent, standing, and slagging off for the first time;
secondary purification treatment: scattering a purifying agent into the aluminum liquid subjected to primary slagging-off, stirring, standing, and performing secondary slagging-off;
pouring treatment: pouring the aluminum liquid subjected to secondary purification treatment;
homogenizing: carrying out homogenization annealing treatment on the cast aluminum foil blank;
thermoplastic deformation treatment: and cutting a sample from the homogenized aluminum foil blank, processing the sample into a hot compression sample, and then performing a hot compression simulation test.
Preferably, the temperature of the melting furnace in the primary purification treatment is 740 to 780 ℃.
Preferably, part of the refining agent is covered on the surface of the completely molten aluminum in the primary purification treatment.
Preferably, the heat preservation time in the primary purification treatment is 30min to 50min, and the standing time in the primary purification treatment and the secondary purification treatment is 10min to 20 min.
Preferably, the purifying agent comprises the following components in percentage by mass: NaCl: 29-31%, KCl: 39% -41%, NaF: 2.5% -3.5% of Na3AlF6：6.5％～7.5％，Na2CO3：6.5％～7.5％，Na2SO4：6.5％～7.5％，CaCl2：1.8％～2.2％，Na2SiF6：1.8％～2.2％。
Preferably, the temperature of casting in the casting treatment is 700 ℃ to 730 ℃.
Preferably, the annealing temperature in the homogenization treatment is 550-570 ℃, and the heat preservation time is 12-15 hours.
Preferably, the deformation temperature in the thermoplastic deformation treatment is 380 ℃ to 420 ℃.
A method for evaluating the purification effect after purification treatment in the method for preparing and purifying the aluminum foil blank is characterized by comprising the following steps of:
determination of impurity content: adding an impurity measuring agent into an aluminum ingot sample block, measuring the mass difference between the original mass of the sample block and the mass after impurity measurement, and calculating the mass percentage of the mass difference to the original mass;
and (3) measuring the impurity removal rate: measuring the impurity content difference between the impurity content without purification treatment and the impurity content after purification treatment, and calculating the percentage of the impurity content difference to the impurity content without purification treatment;
determination of average grain size: the crystal grain sizes were measured by microscopic observation and by a line-cutting method, and the average value was calculated.
Preferably, the number of crystal grains in the measurement of the average size of the crystal grains is 75 to 85, and each crystal grain is located in a different region.
By adopting the technical scheme, the invention has the beneficial effects that: by the preparation and purification treatment method, the original structure and the thermal compression deformation structure form of the aluminum foil blank are more effectively improved, and the mechanical property of the aluminum foil blank material is finally improved, so that the aluminum foil blank has high purity, less impurities, smaller grain structure size and uniform distribution.
Drawings
FIG. 1 is a schematic flow diagram of a preparative purification process according to the present invention;
FIG. 2 is a schematic flow chart of the purification effect evaluation method according to the present invention;
FIG. 3 is a schematic representation of the dimensions of a thermally compressed sample in a thermoplastic deformation process according to the present invention;
FIG. 4a is a metallographic image showing the morphology of the ingot structure in comparative example 1 according to the present invention;
FIG. 4b is a metallographic image showing the morphology of the deformed structures in comparative example 1 according to the present invention;
FIG. 5a is a metallographic image showing the morphology of the ingot structure in comparative example 2 according to the present invention;
FIG. 5b is a metallographic image showing the morphology of the deformed structures in comparative example 2 according to the present invention;
FIG. 6a is a metallographic image showing the morphology of the ingot structure in comparative example 3 according to the present invention;
FIG. 6b is a metallographic image showing the morphology of the deformed structures in comparative example 3 according to the present invention;
FIG. 7a is a metallographic image of the texture of an ingot in example 1 of the present invention;
FIG. 7b is a metallographic image of a deformed texture in example 1 of the present invention;
Detailed Description
The invention is further described below with reference to the figures and the specific embodiments.
According to the invention, the preparation and purification treatment method of the aluminum foil blank
As shown in fig. 1, includes: primary purification treatment: putting the aluminum foil blank into a smelting furnace, controlling the furnace temperature at 760 ℃, adding a purifying agent and a refining agent, adding the purifying agent when an aluminum block is just melted, so that melting and purification are carried out simultaneously to achieve the effect of full purification, adding the refining agent in an amount of 2% based on the mass of the aluminum liquid, and covering part of the refining agent on the surface of the completely melted aluminum liquid; the air-proof structure plays a role in isolating the atmosphere and prevents interference with the outside air; reacting the rest of the raw materials with the aluminum slag, taking the aluminum slag out of the surface of the aluminum liquid, uniformly melting, preserving heat for 40 minutes, adding a degasifier which is mainly hexachloroethane, NaCl and KCl in equal proportion, standing for 15 minutes, and then carrying out primary slagging-off;
secondary purification treatment: scattering a purifying agent into the aluminum liquid subjected to primary slagging-off and stirring at the same time, adding a refining agent at the moment, adding the refining agent in an amount of 1% based on the mass of the aluminum liquid, standing for 15 minutes, and then carrying out secondary slagging-off;
pouring treatment: pouring the aluminum liquid subjected to secondary purification treatment; the temperature during pouring is 720 ℃;
homogenizing: carrying out homogenization annealing treatment on the cast aluminum foil blank; the annealing temperature is 560 ℃, the heat preservation time is 13 hours, and the air cooling is carried out.
Thermoplastic deformation treatment: a sample is cut from the homogenized aluminum foil blank and processed into a cylindrical thermal compression sample with the diameter of 10 multiplied by 12mm on a lathe, two end faces of the sample are processed into small grooves for storing lubricant, a thermal compression simulation test is carried out on a Gleeble-1500 dynamic thermal/mechanical thermal simulator, the deformation temperature is designed to be 400 ℃, the strain rate at each temperature is 0.1s < -1 >, and the compression deformation amount is 50%.
The purifying agent comprises the following components in percentage by mass: NaCl: 30%, KCl: 401%, NaF: 3% of Na3AlF6：7％，Na2CO3：7％，Na2SO4：75％，CaCl2：2％，Na2SiF6：2％。
Preparation of a metallographic phase: and (4) cutting out metallographic samples (cast ingots and samples after plastic deformation), grinding the metallographic samples by using water-milled metallographic abrasive paper, and polishing the metallographic samples on a PG-Z type metallographic sample polishing machine. And cleaning the polished wafer by using clear water, sucking surface water by using filter paper, observing the wafer by using a horizontal metallographic microscope, and shooting the crystal grain structure after casting and plastic deformation. And then carrying out electrolytic polishing and anodizing film coating on the metallographic sample, and observing the appearance of the crystal grains.
The invention relates to a method for evaluating the purification effect
In order to evaluate the effect after the purification treatment, the test takes the determination of the content of the inclusions in the aluminum ingot as an important investigation index. The impurity content is measured by a flux washing method, and the impurity measuring agent mainly comprises NaCl and KCl and contains a small amount of NaF and Na3AlF6, wherein the dosage of the impurity measuring agent is 10 times of the weight of the sample.
Determination of impurity content: adding an impurity measuring agent into an aluminum ingot sample block, measuring the mass difference between the original mass of the sample block and the mass after impurity measurement, and calculating the mass percentage of the mass difference to the original mass;
and (3) measuring the impurity removal rate: measuring the impurity content difference between the impurity content without purification treatment and the impurity content after purification treatment, and calculating the percentage of the impurity content difference to the impurity content without purification treatment;
determination of average grain size: and observing the grains at the edges and the middle parts of the homogenized metallographic specimen and the thermally compressed half-moon metallographic specimen by using a reading microscope. The macroscopic grain size of the material was measured by the line intercept method. When the average grain size is measured by using a line cutting method, the number of grains cut by each test line and the times of cutting by selecting different areas are required to be as many as possible so as to ensure that the measurement result is more accurate. In the experiment, the sizes of 80 crystal grains are measured, then the average value is obtained, and when the crystal grains are observed by a microscope, the multiple of the microscope is the required matching multiple.
The purification treatment method of the present invention will be described with reference to examples
Comparative example 1
(1) Aluminum foil blank raw materials are adopted, and melt purification treatment is not carried out;
(2) carrying out homogenizing annealing treatment, wherein the annealing temperature is 560 ℃, the heat preservation time is 13 hours, and air cooling;
(3) metallographic preparation and observation, as shown in fig. 4 a;
(4) analyzing the purification effect;
(5) thermoplastic deformation, strain rate of 0.1s-1, deformation temperature of 400 ℃ and deformation amount of 50 percent.
(6) Plastic deformation metallographic preparation and observation as shown in fig. 4 b;
comparative example 2
(1) Adopting aluminum foil blank raw materials, adopting a general just-bang refining agent to treat a melt, and blowing argon to remove gas;
(2) carrying out homogenizing annealing treatment, wherein the annealing temperature is 560 ℃, the heat preservation time is 13 hours, and air cooling;
(3) metallographic preparation and observation, as shown in fig. 5 a;
(4) analyzing the purification effect;
(5) thermoplastic deformation, strain rate of 0.1s-1, deformation temperature of 400 ℃ and deformation amount of 50 percent.
(6) Plastic deformation metallographic preparation and observation as shown in fig. 5 b;
comparative example 3
(1) Adopting aluminum foil blank raw materials, adopting a normal-position refining agent to treat a melt, blowing argon gas to remove gas, and filtering aluminum liquid by using a double-stage filter plate;
(2) carrying out homogenizing annealing treatment, wherein the annealing temperature is 560 ℃, the heat preservation time is 13 hours, and air cooling;
(3) metallographic preparation and observation, as shown in fig. 6 a;
(4) analyzing the purification effect;
(5) thermoplastic deformation, strain rate of 0.1s-1, deformation temperature of 400 ℃ and deformation amount of 50 percent.
(6) Plastic deformation metallographic preparation and observation as shown in fig. 6 b;
example 1
(1) Aluminum foil blank raw materials are adopted, and an independently developed purification treatment process is adopted for carrying out aluminum melt purification treatment;
(2) carrying out homogenizing annealing treatment, wherein the annealing temperature is 560 ℃, the heat preservation time is 13 hours, and air cooling;
(3) metallographic preparation and observation, as shown in fig. 7 a;
(4) analyzing the purification effect;
(5) thermoplastic deformation, strain rate of 0.1s-1, deformation temperature of 400 ℃ and deformation amount of 50 percent.
(6) Plastic deformation metallographic preparation and observation as shown in fig. 7 b;
the following is a table showing the purification effect of each comparative example and each example
From the above, it can be seen that the microstructure of the aluminum foil stock in the untreated condition was not uniform (see fig. 4a in proportion 1), the amount of inclusions was large and the distribution was concentrated, the inclusion content was high, and the average size of the inclusions was large (see the analysis table of the purification effect). Through the refining purification treatment and the conventional refining and filtering treatment, the inclusions are obviously reduced and are uniformly distributed, and the structure becomes more uniform (refer to a figure 5a of a comparative example 2 and a figure 6a of a comparative example 3). In the independently developed purification process, the impurity removal and purification effect is optimal, the finer the crystal grain is, the higher the plasticity and toughness is, and the better the mechanical property of the material is.
After plastic deformation, the hot deformed structure according to comparative example 1, fig. 4b and comparative example 2, fig. 5b, has coarse and extremely irregular grains, and a portion of the grains have a distinct elongated shape and the grain structure is not uniform in thickness. Comparative example 3 the grains of fig. 6b are finer, a small fraction of the grains have a clearly elongated shape and the grain structure is more uniform. In example 4, the structure had a fine crystal grain size and a uniform size distribution, and few crystal grains were elongated (see fig. 7a and 7b and a table for analysis of the purification effect). Therefore, the independently developed purification treatment process can more effectively improve the original structure and the thermal compression deformation structure form of the aluminum foil blank, and finally improve the mechanical property of the aluminum foil blank material.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the invention, and all equivalent changes and modifications made in the claims of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation and purification treatment method of the aluminum foil blank is characterized by comprising the following steps of:
primary purification treatment: putting the aluminum foil blank into a smelting furnace, adding a purifying agent and a refining agent, taking the aluminum slag out of the surface of the aluminum liquid, uniformly melting, preserving heat, adding a degassing agent, standing, and slagging off for the first time;
secondary purification treatment: scattering a purifying agent into the aluminum liquid subjected to primary slagging-off, stirring, standing, and performing secondary slagging-off;
pouring treatment: pouring the aluminum liquid subjected to secondary purification treatment;
homogenizing: carrying out homogenization annealing treatment on the cast aluminum foil blank;
thermoplastic deformation treatment: and cutting a sample from the homogenized aluminum foil blank, processing the sample into a hot compression sample, and then performing a hot compression simulation test.
2. The method for manufacturing and purifying aluminum foil stock as claimed in claim 1, wherein the temperature of the melting furnace in the primary purification treatment is 740 to 780 ℃.
3. The method for preparing and purifying aluminum foil stock as claimed in claim 1, wherein a portion of the refining agent is coated on the surface of the completely melted aluminum liquid in the primary purification treatment.
4. The method as claimed in claim 1, wherein the first cleaning process is performed for 30-50 min, and the first cleaning process and the second cleaning process are performed for 10-20 min.
5. The method for preparing and purifying the aluminum foil blank as claimed in claim 1, wherein the purifying agent comprises the following components in percentage by mass: NaCl: 29-31%, KCl: 39% -41%, NaF: 2.5% -3.5% of Na3AlF6：6.5％～7.5％，Na2CO3：6.5％～7.5％，Na2SO4：6.5％～7.5％，CaCl2：1.8％～2.2％，Na2SiF6：1.8％～2.2％。
6. The method for preparing and purifying aluminum foil stock as claimed in claim 1, wherein the casting temperature in the casting process is 700 ℃ to 730 ℃.
7. The method for preparing and purifying the aluminum foil blank as claimed in claim 1, wherein the annealing temperature in the homogenization treatment is 550-570 ℃, and the holding time is 12-15 hours.
8. The method for preparing and purifying aluminum foil stock as claimed in claim 1, wherein the deformation temperature in the thermoplastic deformation treatment is 380-420 ℃.
9. A method for evaluating a purification effect after a purification treatment in a purification treatment method for manufacturing an aluminum foil blank according to any one of claims 1 to 8, comprising:
determination of impurity content: adding an impurity measuring agent into an aluminum ingot sample block, measuring the mass difference between the original mass of the sample block and the mass after impurity measurement, and calculating the mass percentage of the mass difference to the original mass;
and (3) measuring the impurity removal rate: measuring the impurity content difference between the impurity content without purification treatment and the impurity content after purification treatment, and calculating the percentage of the impurity content difference to the impurity content without purification treatment;
determination of average grain size: the crystal grain sizes were measured by microscopic observation and by a line-cutting method, and the average value was calculated.
10. The method according to claim 9, wherein the number of the crystal grains in the measurement of the average size of the crystal grains is 75 to 85, and each crystal grain is located in a different region.
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